WO2017190572A1 - Pile rechargeable et son procédé de préparation - Google Patents

Pile rechargeable et son procédé de préparation Download PDF

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Publication number
WO2017190572A1
WO2017190572A1 PCT/CN2017/079275 CN2017079275W WO2017190572A1 WO 2017190572 A1 WO2017190572 A1 WO 2017190572A1 CN 2017079275 W CN2017079275 W CN 2017079275W WO 2017190572 A1 WO2017190572 A1 WO 2017190572A1
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Prior art keywords
lithium
carbonate
positive electrode
secondary battery
battery
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Ceased
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PCT/CN2017/079275
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English (en)
Chinese (zh)
Inventor
唐永炳
圣茂华
张帆
季必发
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Shenzhen Institute of Advanced Technology of CAS
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Shenzhen Institute of Advanced Technology of CAS
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Priority to US15/777,950 priority Critical patent/US20180342758A1/en
Priority to EP17792399.2A priority patent/EP3370294B1/fr
Priority to KR1020187012965A priority patent/KR20180066169A/ko
Priority to JP2018521881A priority patent/JP6896725B2/ja
Priority to CN201780001704.2A priority patent/CN107615550B/zh
Priority to KR1020217021610A priority patent/KR20210088770A/ko
Publication of WO2017190572A1 publication Critical patent/WO2017190572A1/fr
Anticipated expiration legal-status Critical
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Definitions

  • the present invention relates to the field of batteries, and in particular to a secondary battery and a method of fabricating the same.
  • Lithium-ion batteries are the first choice for power supply in today's electronic products due to their high specific capacity, long cycle life and high cost performance.
  • the core components of a lithium ion battery typically contain a positive electrode, a negative electrode, and an electrolyte.
  • the commercial lithium ion battery uses a transition metal oxide or a polyanionic metal compound as a positive electrode active material, graphite or carbon as a negative electrode active material, and an ester electrolyte as an electrolyte.
  • graphite as the negative active material, graphite occupies a large part of the volume and weight in the battery, which limits the battery capacity and energy density of the lithium ion battery, and increases the complexity of the production process and the production cost.
  • the present invention provides a secondary battery and a preparation method thereof, which aim to solve the problem that the existing lithium battery uses graphite as a negative electrode active material, the battery capacity and energy density of the battery are low, and the production process is complicated, and the production is complicated. The problem of higher costs.
  • the present invention provides a secondary battery including a battery negative electrode, an electrolyte, a separator, and a battery positive electrode, wherein
  • the battery negative electrode includes a negative electrode current collector; the negative electrode current collector includes a metal or metal alloy or a metal composite conductive material, and the negative electrode current collector simultaneously serves as a negative electrode active material;
  • the electrolyte includes an electrolyte and a solvent, and the electrolyte is a lithium salt;
  • the battery positive electrode includes a positive electrode current collector and a positive electrode active material layer, and the positive electrode active material layer package A positive active material capable of reversibly deintercalating lithium ions, the positive current collector comprising a metal, a metal alloy or a metal composite conductive material.
  • the positive electrode active material includes lithium cobaltate, lithium nickelate, lithium manganate, lithium iron phosphate, lithium nickel cobaltate binary material, spinel structure lithium manganese oxide, lithium nickel cobalt manganese oxide ternary material. a composite material of one or more or one of layered lithium-rich and high manganese materials.
  • the anode current collector includes one of aluminum, magnesium, lithium, vanadium, copper, iron, tin, zinc, nickel, titanium, manganese, or a composite of any one of them, or any one of them Alloy.
  • the anode current collector is aluminum.
  • the structure of the anode current collector is an aluminum foil, or a porous aluminum, or a porous aluminum coated with a carbon material, or a multilayer composite structure of aluminum.
  • the cathode current collector includes one of aluminum, magnesium, lithium, vanadium, copper, iron, tin, zinc, nickel, titanium, manganese, or a composite of any one of them, or any one of them Alloy
  • the cathode current collector is preferably aluminum.
  • the electrolyte includes, but is not limited to, lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium acetate, lithium salicylate, lithium acetoacetate, lithium carbonate, lithium trifluoromethanesulfonate, lithium lauryl sulfate
  • lithium citrate lithium bis(trimethylsilyl)amide, lithium hexafluoroarsenate, and lithium trifluoromethanesulfonimide
  • concentration of the electrolyte is from 0.5 to 2 mol/L.
  • the solvent includes one or more of an ester, a sulfone, an ether, a nitrile organic solvent, or an ionic liquid.
  • the solvent comprises propylene carbonate, ethylene carbonate, butylene carbonate, diethyl carbonate, dimethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, methyl propyl carbonate, dibutyl carbonate, Butyl carbonate, methyl isopropyl carbonate, methyl ester, methyl formate, methyl acetate, N,N-dimethylacetamide, vinyl fluorocarbonate, methyl propionate, ethyl propionate, ethyl acetate Ester, ⁇ -butyrolactone, tetrahydrofuran, 2-methyl Tetrahydrofuran, 1,3-dioxocyclopentane, 4-methyl-1,3-dioxocyclopentane, dimethoxymethane, 1,2-dimethoxyethane, 1,2-dimethoxypropane
  • the electrolyte further includes an additive including one or more of an ester, a sulfone, an ether, a nitrile or an olefin organic additive.
  • the additive comprises fluoroethylene carbonate, vinylene carbonate, ethylene carbonate, 1,3-propane sultone, 1,4-butane sultone, vinyl sulphate, propylene sulfate Ester, ethylene sulfate, vinyl sulfite, propylene sulfite, dimethyl sulfite, diethyl sulfite, ethylene sulfite, methyl chloroformate, dimethyl sulfoxide, benzene Methyl ether, acetamide, diazabenzene, m-diazabenzene, crown ether 12-crown-4, crown ether 18-crown-6, 4-fluoroanisole, fluorochain ether, difluoromethyl Ethylene carbonate, trifluoromethyl ethylene carbonate, vinyl chlorocarbonate, vinyl bromoacetate, trifluoroethylphosphonic acid, bromobutyrolactone, fluoroacet
  • the additive is vinylene carbonate in an amount of 5% by weight.
  • the positive electrode active material layer further comprises a conductive agent and a binder
  • the positive electrode active material is contained in an amount of 60 to 95% by weight
  • the conductive agent is contained in an amount of 0.1 to 30% by weight
  • the binder is contained in an amount of 0.1 to 10% by weight. %.
  • the present invention also provides a method for preparing the above secondary battery, comprising:
  • Preparing a battery negative electrode cutting a metal, or a metal alloy, or a metal composite conductive material into a desired size, and washing it as a battery negative electrode, the metal or metal alloy or metal composite conductive material simultaneously serving as a negative current collector and Anode active material;
  • the positive electrode of the battery weigh the positive active material, the conductive agent and the binder according to a certain ratio, and add it to a suitable solvent to fully grind into a uniform slurry; take a metal or metal alloy or a metal composite conductive material, and wash the surface thereof As a positive electrode current collector; then uniformly coating the slurry on the surface of the positive electrode collector, and then cutting the slurry to form a positive electrode active material layer, and then cutting to obtain a battery positive electrode of a desired size;
  • the battery negative electrode, the electrolytic solution, the separator, and the battery positive electrode were assembled in this order to obtain a secondary battery.
  • the invention has the advantages that the traditional anode active material is eliminated, the weight, volume and manufacturing cost of the battery are effectively reduced, and the production process is simplified; the metal or metal alloy or metal composite is eliminated.
  • the negative electrode current collector is simultaneously used as the negative electrode active material, which effectively increases the capacity of the battery; the energy density of the battery is remarkably improved by the reduction of the weight and volume of the battery and the increase of the battery capacity, and the battery has a good charge and discharge cycle. performance.
  • FIG. 1 is a schematic structural view of a secondary battery according to an embodiment of the present invention.
  • FIG. 1 is a schematic structural diagram of a secondary battery according to an embodiment of the present invention.
  • a secondary battery according to an embodiment of the present invention includes a battery negative electrode 1, an electrolyte 2, a separator 3, a battery positive electrode (including a positive electrode active material layer 4 and a positive electrode current collector 5); wherein the battery negative electrode 1 includes a negative electrode set a fluid, the anode current collector comprising a metal or metal alloy or a metal composite conductive material, the anode current collector simultaneously serving as a negative electrode active material; the electrolyte 2 includes an electrolyte and a solvent, the electrolyte is a lithium salt; and the battery positive electrode includes a positive electrode current collector 5 And a positive electrode active material layer 4 comprising a metal or metal alloy or a metal composite conductive material, the positive active material layer comprising a positive active material capable of reversibly deintercalating lithium ions.
  • the working principle of the battery provided by the embodiment of the present invention is: the secondary battery provided by the embodiment of the present invention does not contain the negative active material, and during the charging process, the positive active material desorbs lithium ions, and the negative current collector metal or metal alloy or The composite material is alloyed to form a lithium-metal alloy. During the discharge process, the lithium-metal alloy is decomposed into lithium ions and embedded in the positive electrode active material to realize the charge and discharge process.
  • the reaction of the negative electrode is different.
  • the reaction of the conventional lithium ion battery is the insertion-extraction reaction of lithium ions, and the negative electrode of the secondary battery of the present invention occurs. It is an alloy-de-alloying reaction of lithium ions.
  • the battery provided by the embodiment of the invention does not need the traditional negative active material, which reduces the volume and cost; at the same time, the alloying reaction between the metal and the lithium ion has a larger battery capacity, the weight and volume of the battery are reduced, and the battery capacity is improved. Significantly increases the energy density of the battery, and saves production costs and simplifies the production process.
  • LiCoO 2 lithium cobaltate
  • LiNiO 2 lithium nickelate
  • LiMn 2 O 4 lithium manganate
  • the anode current collector includes, but is not limited to, an alloy or a metal composite of one or any one of aluminum, magnesium, lithium, vanadium, copper, iron, tin, zinc, nickel, titanium, manganese. Things.
  • the cathode current collector includes, but is not limited to, an alloy or a metal composite of one or any one of aluminum, magnesium, lithium, vanadium, copper, iron, tin, zinc, nickel, titanium, manganese. Things.
  • the anode current collector is aluminum.
  • the cathode current collector is aluminum.
  • the solvent in the electrolytic solution is not particularly limited as long as the solvent can dissociate the electrolyte into cations and anions, and the cations and anions can freely migrate.
  • the solvent of the examples of the present invention is an ester, a sulfone, an ether, a nitrile organic solvent or an ionic liquid.
  • Solvents include, but are not limited to, propylene carbonate, ethylene carbonate, butylene carbonate, diethyl carbonate, dimethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, methyl propyl carbonate, dibutyl carbonate, carbonic acid Butyl ester, isopropyl carbonate, methyl ester, methyl formate, methyl acetate, N,N-dimethylacetamide, fluoroethylene carbonate, methyl propionate, ethyl propionate, ethyl acetate, ⁇ -butyrolactone, tetrahydrofuran, 2-methyltetrahydrofuran, 1,3-dioxocyclopentane, 4-methyl-1,3-dioxocyclopentane, dimethoxymethane, 1,2-dimethyl Oxyethane, 1,2-dimethoxypropane, triethylene glycol dimethyl ether, dimethyl sulfone, dimethyl
  • the electrolyte in the examples further includes an additive including, but not limited to, fluoroethylene carbonate, vinylene carbonate, ethylene carbonate, 1,3-propane sultone, 1,4-butane sultone.
  • the content of the additive is from 0.1 to 20% by weight, further from 1 to 5% by weight.
  • the additive added to the electrolyte can form a stable solid electrolyte membrane on the surface of the anode current collector, so that the anode current collector is not destroyed when reacted as an active material, and its function and shape can be maintained, and the number of cycles of the battery can be improved.
  • the additive is vinylene carbonate in an amount of 5% by weight.
  • the positive electrode active material layer further includes a conductive agent and a binder
  • the positive electrode active material is contained in an amount of 60 to 95% by weight
  • the conductive agent is contained in an amount of 0.1 to 30% by weight
  • the binder is contained in an amount of 0.1 to 10% by weight. %.
  • the conductive agent and the warrant agent are not particularly limited and may be used in the art.
  • the conductive agent is one or more of conductive carbon black, Super P conductive carbon sphere, conductive graphite KS6, carbon nanotube, conductive carbon fiber, graphene, and reduced graphene oxide.
  • the binder is one or more of polyvinylidene fluoride, polytetrafluoroethylene, polyvinyl alcohol, carboxymethyl cellulose, SBR rubber, and polyolefin.
  • the anode current collector is a multilayer composite of porous aluminum or aluminum coated with aluminum foil or porous aluminum or carbon material.
  • the lithium ion which uses the porous aluminum foil to remove the positive active material is more fully reacted with the metal aluminum alloy, and the battery capacity is improved; the porous aluminum structure coated with the carbon material improves the battery capacity, and is protected by the carbon material coating layer.
  • the effect is beneficial to maintain the structural stability of the aluminum and further improve the cycle stability of the battery; the use of the aluminum multilayer composite material is also beneficial for suppressing and improving the volume expansion effect of the aluminum foil and improving the cycle performance of the battery.
  • the composition of the separator used in the secondary battery provided by the embodiment of the present invention is an insulated porous
  • the polymer film or the inorganic porous film includes one or more of a porous polypropylene film, a porous polyethylene film, a porous composite polymer film, a glass fiber-based film, or a porous ceramic separator.
  • the function of the separator is to physically isolate the positive and negative electrodes of the battery from short circuits while allowing ions in the electrolyte to pass freely.
  • the embodiment of the present invention further provides a method for preparing the above secondary battery, comprising:
  • Step 101 Prepare a battery negative electrode, cut a metal or metal alloy or a metal composite conductive material into a desired size, and then wash the surface of the cut metal conductive material, and use the washed metal conductive material as a negative electrode set.
  • the fluid is used as a battery negative electrode.
  • Step 102 Prepare an electrolyte solution, and weigh a certain amount of electrolyte into the corresponding solvent, and fully stir and dissolve.
  • Step 103 Prepare a separator, cut a porous polymer film, an inorganic porous film or a glass fiber-based film into a desired size, and clean it.
  • Step 104 preparing a positive electrode of the battery, weighing a living active material, a conductive agent and a binder according to a certain ratio, adding a suitable slurry to a uniform slurry to form a positive active material layer; and forming a metal or a metal alloy or a metal composite
  • the surface of the conductive material is washed as a positive electrode current collector; then the positive electrode active material layer is uniformly applied to the surface of the positive electrode current collector, and after the positive electrode active material layer is completely dried, it is cut to obtain a battery positive electrode of a desired size.
  • Step 105 assembling using the battery negative electrode, the electrolyte solution, the separator, and the battery positive electrode.
  • the metal conductive material in step 101 is an alloy or metal of one or any one of aluminum, magnesium, lithium, vanadium, copper, iron, tin, zinc, nickel, titanium, manganese. Complex.
  • the electrolyte in the step 102 is a lithium salt
  • the solvent includes an ester, a sulfone, an ether or a nitrile organic solvent.
  • the electrolyte is prepared, further comprising: adding an additive to the solvent for stirring.
  • the solvent includes, but is not limited to, one or more of ethylene carbonate, diethyl carbonate, dimethyl carbonate, and ethyl methyl carbonate; the additive is vinylene carbonate, ethylene sulfite, propylene sulfite, Sulfuric acid One or more of ethylene ester cyclobutyl sulfone, 1,3-dioxocyclopentane, acetonitrile or long-chain olefin.
  • the positive electrode active material in step 104 is one or more selected from the group consisting of lithium cobaltate, lithium manganate, lithium titanate, lithium nickel cobalt manganese oxide or lithium iron phosphate.
  • Metal conductive materials include, but are not limited to, alloys or metal composites of one or any of aluminum, magnesium, lithium, vanadium, copper, iron, tin, zinc, nickel, titanium, manganese.
  • the step 105 is performed by using the battery negative electrode, the electrolyte, the separator, and the battery positive electrode, and specifically includes: preparing the negative electrode, the separator, and the battery under an inert gas or an anhydrous oxygen-free environment.
  • the positive electrodes are closely stacked in sequence, and the electrolyte is added to completely infiltrate the separator, and then packaged into the battery case to complete the battery assembly.
  • steps 101-104 describe the operation of the preparation method of the present invention in a specific order, it is not required or implied that these operations must be performed in this particular order.
  • the preparation of steps 101-104 can be performed simultaneously or in any order.
  • the secondary battery preparation method and the foregoing secondary battery are based on the same inventive concept, and the secondary battery obtained by the secondary battery preparation method has all the effects of the foregoing secondary battery, and details are not described herein again.
  • Preparation of battery negative electrode Take aluminum foil with a thickness of 0.02 mm, cut into a 12 mm diameter disc, wash the aluminum foil with ethanol, and dry it as a negative current collector for use.
  • the glass fiber paper was cut into a 16 mm diameter disc and dried for use as a separator.
  • Formulation of electrolyte 1.5 g of lithium hexafluorophosphate (concentration: 1 mol/L) was added to 3.2 mL of ethylene carbonate, 3.2 mL of dimethyl carbonate and 3.2 mL of ethyl methyl carbonate in a mixed solvent, and the mass content was added. 5% of vinylene carbonate (0.545 g) was used as an additive, and the mixture was thoroughly stirred until lithium hexafluorophosphate was completely dissolved, and it was used as an electrolyte.
  • Preparation of battery positive electrode 0.4 g of lithium cobaltate, 0.05 g of carbon black, 0.05 g of polyvinylidene fluoride was added to 2 mL of nitromethylpyrrolidone solution, and fully ground to obtain a uniform slurry; then the slurry was uniformly coated on the surface of the aluminum foil and Dry in vacuum. The electrode sheet obtained by drying was cut into a disk having a diameter of 10 mm, and compacted as a battery positive electrode.
  • the prepared negative electrode current collector, separator, and battery positive electrode are closely stacked in sequence, and the electrolyte is dripped to completely infiltrate the separator, and then the stacked portion is packaged into the button battery case. , complete battery assembly.
  • the battery negative electrode take 0.4g graphite, 0.05g carbon black, 0.05g polyvinylidene fluoride into 2mL nitromethylpyrrolidone solution, fully grind to obtain a uniform slurry; then uniformly apply the slurry to the surface of aluminum foil and vacuum dry .
  • the electrode sheet obtained by drying was cut into a disk having a diameter of 10 mm, and compacted as a battery negative electrode.
  • the polymer polyethylene was cut into a disk having a diameter of 16 mm, and dried for use as a separator.
  • the electrolyte was prepared: 0.75 g of lithium hexafluorophosphate was weighed and added to 2.5 mL of ethylene carbonate and 2.5 mL of dimethyl carbonate, and the mixture was thoroughly stirred until lithium hexafluorophosphate was completely dissolved, and then it was used as an electrolyte.
  • Preparation of battery positive electrode 0.4 g of lithium cobaltate positive electrode material, 0.05 g of carbon black, 0.05 g of polyvinylidene fluoride was added to 2 mL of nitromethylpyrrolidone solution, and fully ground to obtain a uniform slurry; then the slurry was uniformly coated on aluminum foil. The surface was dried under vacuum. The electrode sheet obtained by drying was cut into a disk having a diameter of 10 mm, and compacted as a battery positive electrode.
  • the prepared negative electrode current collector is separated in an inert gas-protected glove box.
  • the membrane and the positive electrode of the battery are closely stacked in sequence, and the electrolyte is dripped to completely infiltrate the separator, and then the stacked portion is packaged into the button battery case to complete the battery assembly.
  • the secondary battery prepared in the above embodiment of the secondary battery preparation method was charged by a constant current of 100 mA/g of the positive electrode active material until its voltage reached 4.2 V, and then discharged at the same current until the voltage reached 3V, measuring its battery capacity and energy density, testing its cycle stability, expressed in cycles, the number of cycles is the number of times the battery is charged and discharged when the battery capacity is attenuated to 85%.
  • Example 1 of the present invention The electrochemical performance test of the battery of the secondary battery provided in Example 1 of the present invention was compared with the performance of the conventional lithium ion battery mentioned in the background, and the results and comparisons are shown in Table 1.
  • the secondary battery of the first embodiment of the present invention has no graphite compared with the conventional lithium ion battery, the raw material cost and the process cost are lowered, and the energy density of the battery is further improved.
  • Embodiments 19-29 are the same as the steps of the preparation process of the secondary battery of Example 1, except that the selection of the positive electrode active material is different, as shown in Table 3.
  • Examples 30-45 are the same as the secondary battery preparation process steps of Example 1, except that the electrolyte salts are different, as shown in Table 4.
  • Examples 46-50 are the same as the secondary battery preparation process steps of Example 1, except that the electrolyte salt concentration is different, see Table 5 for details.
  • Examples 51-94 are the same as the secondary battery preparation process steps of Example 1, except that the types of solvents in the electrolyte are different, as shown in Table 6.
  • Examples 95-145 are the same as the secondary battery preparation process steps of Example 1, except that the types of additives in the electrolyte are different, as shown in Table 7.
  • Examples 145-151 are the same as the secondary battery preparation process steps of Example 1, except that the content of the additive in the electrolyte is different, as shown in Table 8.
  • Examples 152-153 are the same as the secondary battery preparation process steps of Example 1, except that the types of the separators are different, see Table 9 for details.
  • the separator can be selected from a conventional separator, and both of the secondary batteries of the present invention can obtain better cycle performance and higher energy density.
  • Examples 154-159 are the same as the secondary battery preparation process steps of Example 1, except that the active material, the conductive agent, the binder type, and the mass percentage in the positive electrode material are different. See Table 10 for details.
  • Embodiments 160-172 are the same as the secondary battery preparation process steps of Example 1, except that the types of the positive current collectors are different, as shown in Table 11.

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Abstract

La présente invention concerne le domaine des piles, et plus précisément une pile rechargeable et son procédé de préparation. La pile rechargeable comprend une électrode négative de pile, un liquide électrolytique, une membrane et une électrode positive de pile, l'électrode négative de pile comprenant un collecteur de courant d'électrode négative, et le collecteur de courant d'électrode négative servant également de matériau actif d'électrode négative; le liquide électrolytique comprenant un électrolyte et un solvant, l'électrolyte étant un sel de lithium; l'électrode positive de pile comprenant un collecteur de courant d'électrode positive et une couche de matériau actif d'électrode positive, la couche de matériau actif d'électrode positive comprenant un matériau actif d'électrode positive pouvant désintercaler de manière réversible des ions lithium. Dans la présente invention, étant donné qu'un métal ou alliage métallique ou composite métallique est utilisé simultanément comme collecteur de courant d'électrode négative et comme matériau actif d'électrode négative, aucun matériau actif d'électrode négative supplémentaire ne doit être ajouté, ce qui réduit efficacement le poids et le volume de la pile; et par ailleurs, la capacité de la pile est efficacement augmentée. En outre, la densité d'énergie de la pile est considérablement améliorée, le coût de production est réduit, le procédé de production est simplifié, et la pile rechargeable de la présente invention présente de bonnes performances de cycle de charge et de décharge.
PCT/CN2017/079275 2016-05-06 2017-04-01 Pile rechargeable et son procédé de préparation Ceased WO2017190572A1 (fr)

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US15/777,950 US20180342758A1 (en) 2016-05-06 2017-04-01 Secondary battery and preparation method therefor
EP17792399.2A EP3370294B1 (fr) 2016-05-06 2017-04-01 Pile rechargeable et son procédé de préparation
KR1020187012965A KR20180066169A (ko) 2016-05-06 2017-04-01 이차 전지 및 그 제조방법
JP2018521881A JP6896725B2 (ja) 2016-05-06 2017-04-01 二次電池及びその製造方法
CN201780001704.2A CN107615550B (zh) 2016-05-06 2017-04-01 一种二次电池及其制备方法
KR1020217021610A KR20210088770A (ko) 2016-05-06 2017-04-01 이차 전지 및 그 제조 방법

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